摘要
目的评估6种分析保护剂[L-古洛糖酸-γ-内酯、D-山梨糖醇、莽草酸、3-乙氧基-1,2丙二醇、D-泛醇、二(2-羟乙基)亚氨基三(羟基)甲烷]在气相色谱-串联质谱(gas chromatography-tandem mass spectrometry,GC-MS/MS)技术中对果蔬农药残留检测基质效应(matrix effect,ME)的补偿效能,并用于检测果蔬中45种农药残留。方法在单因素实验基础上,设计正交试验对复合保护剂配方进行优化。使用SPSS Statistics 27软件对单因素实验结果和复合实验结果进行计算和统计分析,评估各分析保护剂单独使用时不同浓度对ME影响,以及复合使用时不同浓度对ME的影响,选择出理想的复合分析保护剂组合。结果采用复合保护剂AP3[上机液质量浓度分别为L-古洛糖酸-γ-内酯0.40 mg/mL、D-山梨糖醇0.40 mg/mL、莽草酸0.40 mg/mL、3-乙氧基-1,2丙二醇1.00 mg/mL、D-泛醇0.015 mg/mL、二(2-羟乙基)亚氨基三(羟基)甲烷0.015 mg/mL]进行基质匹配标准曲线定量时,能显著改善色谱峰形并实现综合补偿效果。农药在2.5~200.0µg/L线性范围内呈现良好相关性(r2>0.995),冬瓜检出限为0.25~1.95µg/kg,定量限为0.91~5.12µg/kg;梨检出限为0.16~1.87µg/kg,定量限为0.71~5.34µg/kg。选择低、中、高3个添加水平(4、8、20µg/kg),所有目标物回收率均稳定于77.4%~117.6%,符合农药残留分析规范要求。结论相较于GB 23200.113—2018《食品安全国家标准植物源性食品中208种农药及其代谢物残留量的测定气相色谱-质谱联用法》方法,本研究所建方法对45种农药及其代谢物的回收率具有显著提升,其灵敏度与准确度指标满足高通量果蔬样品中农药残留的筛查与定量检测需求。
Objective To evaluate the compensation efficiency of 6 kinds of analytical protectants[L-gulonic acid-γ-lactone,D-sorbitol,shikimic acid,3-ethoxy-1,2 propanediol,D-panthenol and bis(2-hydroxyethyl)iminotri(hydroxymethyl)methane]for the matrix effect(ME)of pesticide residue detection in fruits and vegetables using gas chromatography tandem mass spectrometry(GC-MS/MS)technology,and establish a detection method for 45 kinds of pesticide residues in fruits and vegetables.Methods Based on single-factor experiments,an orthogonal test was designed to optimize the formulation of the composite protective agent.Using SPSS Statistics 27 software,the results of single-factor experiments and composite experiments were calculated and statistically analyzed to evaluate the effects of different concentrations of individual analysis protective agents on ME,as well as the effects of different concentrations when used in combination.The ideal combination of composite protective agents was selected.Results Each when using the composite protective agent AP3[with mass concentrations of L-gulonolactone 0.40 mg/mL,D-sorbitol 0.40 mg/mL,shikimic acid 0.40 mg/mL,3-ethoxy-1,2-propanediol 1.00 mg/mL,D-panthenol 0.015 mg/mL and bis(2-hydroxyethyl)iminotri(hydroxymethyl)methane 0.015 mg/mL]for matrix-matched standard curve quantification,the chromatographic peak shape was significantly improved and comprehensive compensation effects were achieved.The pesticides exhibited excellent correlation within the linear range of 2.5-200.0μg/L(r2>0.995).The limits of detection for winter melon were 0.25-1.95μg/kg,and the limits of quantitation were 0.91-5.12μg/kg;for pear,the limits of detection were 0.16-1.87μg/kg,and the limits of quantitation were 0.71-5.34μg/kg.The 3 spiking levels(4,8 and 20μg/kg)were selected,and the recoveries of all target analytes remained stable at 77.4%-117.6%,meeting the requirements of pesticide residue analysis standards.Conclusion Compared with the GB 23200.113—2018 National food safety standards-Determination of residues of 208 pesticides and their metabolites in plant-based foods-Gas chromatography-mass spectrometry standard method,the method developed in this study has significantly improved the recovery rates of 45 kinds of pesticides and their metabolites.Its sensitivity and accuracy indicators meet the screening and quantitative detection needs of pesticide residues in high-throughput fruit and vegetable samples.
作者
刘小丽
王丽娟
段鹿梅
豆志培
王风英
LIU Xiao-Li;WANG Li-Juan;DUAN Lu-Mei;DOU Zhi-Pei;WANG Feng-Ying(Hebi Product Quality Inspection and Testing Center,Hebi 458000,China;Zhengzhou Product Quality Inspection and Testing Center,Zhengzhou 450008,China;Kaifeng Product Quality Inspection and Testing Center,Kaifeng 475000,China)
出处
《食品安全质量检测学报》
2025年第22期143-151,共9页
Journal of Food Safety and Quality
基金
河南省市场监管局科技项目(HNSCJGK202575)。
关键词
复合分析保护剂
果蔬
农药残留
气相色谱-串联质谱法
composite analysis protective agent
fruits and vegetables
pesticide residues
gas chromatographytandem mass spectrometry
